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Carried catalyst synthesizing diphenyl carbonate and its preparing method

The technology of a supported catalyst and diphenyl carbonate, applied in the field of supported catalyst and its preparation, can solve the problems of low efficiency, unsatisfactory reaction effect, low yield of diphenyl carbonate, etc., and achieves easy recovery and easy separation , the effect of high catalytic activity

Inactive Publication Date: 2003-01-22
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The parent of Rh is RhCl 3 ·H 2 O, the carrier is TiO 2 and rare earth oxides, but the reaction effect is not ideal, and the yield of DPC is only 3%
Despite the many advantages of supported catalysts, the current supported catalysts for the oxidative carbonylation of phenol to diphenyl carbonate are not efficient and yield low diphenyl carbonate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The preparation of embodiment 1 non-precious metal compound supported catalyst

[0025] 1. Grind the carrier HZSM-5 into fine particles in a mortar, use a sieve to obtain HZSM-5 particles with a mesh size of 20-40, place them in a muffle furnace and roast at 550°C for later use;

[0026] 2. Take 5 grams of roasted HZSM-5, and use deionized water to measure the volume of the solution required for equal volume impregnation to 7ml;

[0027] 3. Weigh 0.2500 g of Cu(OAc) 2 , dissolved in 7 ml of ammonia water with a volume percentage of 2%-5%, and left to stand for a period of time until the solution is uniform;

[0028] 4. Add the impregnation solution drop by drop to 5 grams of roasted HZSM-5, and impregnate with equal volume for 14 hours;

[0029] 5. Vacuum dry in a constant temperature water bath at 55°C for 8 hours;

[0030] 6. Calcining the dried catalyst in a muffle furnace at 550° C. for 8 hours to obtain a non-precious metal compound-supported catalyst, which was...

Embodiment 3

[0036] The preparation step of catalyst is identical with embodiment 1, but changes Cu(OAc) 2 The amount of Cu(OAc) in the prepared catalyst 2 The loads vary, as shown in Table 1. The prepared catalyst was used to synthesize diphenyl carbonate by liquid-phase oxidative carbonylation, and the reaction conditions were the same as in Example 2. The catalytic performance is shown in Table 1.

[0037] Table 1 Different Cu(OAc) 2 Effect of Loading Amount on Catalyst Activity

[0038] Cu content / wt% 1 2.5 5 7.5 10

[0039] DPC * Yield / % 2.0 5.6 14.2 13.8 14.1

[0040] * DPC: diphenyl carbonate

Embodiment 4

[0042] The preparation steps of the catalyst were the same as in Example 1, but the carrier of the catalyst was changed, as shown in Table 2. The prepared catalyst was used to synthesize diphenyl carbonate by liquid-phase oxidative carbonylation, and the reaction conditions were the same as in Example 2. The catalytic performance is shown in Table 2.

[0043]Table 2 Effect of different supports on catalyst activity

[0044] Carrier HZSM-5 Hβ Zeolite 4A Molecular Sieve 5A Molecular Sieve

[0045] DPC * Yield / % 14.2 8.6 4.2 4.8

[0046] * DPC: diphenyl carbonate

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Abstract

The present invention provides carried non-mobile metal compound catalyst Cu(OAc)2 / zeolite for synthesizing diphenyl carbonate and its preparation. The catalyst consists of zeolite in 50-100 weight portions and Cu(OAc)2 in 0.1-30 weight portions. It is prepared through equi-volume soaking and roasting at 250-750 deg.C. The catalyst system has metal acetate as inorganic oxidation-reduction assistant, hydroquinone as organic oxidation-reduction assistant, and tetrabutyl ammonium bridge as surfactant. The catalyst has very high catalytic activity and excellent selectivity to liquid phenol in synthesizing diphenyl carbonate. The catalyst is easy to separate from product, easy to recover and regenerate and has simple preparation process.

Description

technical field [0001] The invention relates to a supported catalyst and a preparation method thereof, and relates to a non-precious metal compound supported catalyst Cu(OAc) for synthesizing diphenyl carbonate by phenol liquid-phase oxidative carbonylation 2 / Zeolite and its preparation method. Background technique [0002] Diphenyl carbonate has low toxicity and no pollution. It is an important environmental chemical product and can be used to synthesize many important medicines, pesticides and other organic compounds and polymer materials. The preparation methods of diphenyl carbonate include phosgene method, transesterification method and phenol oxidative carbonylation method. The phosgene method has disadvantages such as complex process, highly toxic raw material phosgene, and serious environmental pollution, and is gradually being eliminated; the transesterification method uses dimethyl carbonate or dimethyl oxalate as raw materials, which has high cost and low react...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07C68/00
Inventor 王延吉赵茜刘宏伟赵新强
Owner HEBEI UNIV OF TECH
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